本文關(guān)鍵詞：海洋用電化學(xué)傳感器的制備及研究　出處：《華東師范大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 海水 Ir/IrO_2pH電極 Ag/Ag_2S H_2S電極 金汞齊電極

【摘要】：21世紀(jì)是海洋世紀(jì),研究海洋環(huán)境中的各種理化性質(zhì)關(guān)乎人類生存和發(fā)展。原位測(cè)試能夠及時(shí)反饋測(cè)試環(huán)境的理化參數(shù)的變化情況,因而是研究海洋的學(xué)者們關(guān)注的熱點(diǎn)。本課題主要制備了幾種具有體積小巧、操作簡單、便于微型化、靈敏度高、可原位測(cè)試等特點(diǎn),并能用于海洋環(huán)境測(cè)試的電化學(xué)傳感器,主要內(nèi)容如下:(1)采用熔融碳酸鹽法和NaOH循環(huán)熱氧化法制備Ir/IrO2 pH電極,并對(duì)電極的表面形貌、成分含量、電極的響應(yīng)時(shí)間、可逆性和穩(wěn)定性等工作性能進(jìn)行綜合分析,認(rèn)為NaOH循環(huán)熱氧化法是較適合的制備Ir/IrO2電極的方法。在此基礎(chǔ)上,首次提出采用水熱水化法改進(jìn)電極的穩(wěn)定性。實(shí)驗(yàn)結(jié)果表明:水熱水化處理后的電極具有響應(yīng)速率快(3s)、靈敏度高(70.5mV/pH)、重復(fù)性好、滯后性小、使用壽命長等優(yōu)點(diǎn)。在長達(dá)一個(gè)多月的連續(xù)測(cè)試中,電勢(shì)漂移小于5 mV。該水熱處理方法有效地解決了Ir/IrO2 pH電極長期以來存在的電勢(shì)漂移現(xiàn)象,提高了電極的穩(wěn)定性。(2)選用Ag絲作為金屬基體,分別采用硫化鈉法、蘸取銀漿法和硫代乙酰胺(CH3CSNH2)法制備Ag/Ag2S電極。并從中篩選出適合海洋環(huán)境使用的Ag/AgaS電極的制備方法。實(shí)驗(yàn)結(jié)果表明:后兩種方法所制備的電極均具有響應(yīng)速率快、靈敏度高、檢測(cè)范圍廣的特點(diǎn),有效改進(jìn)了硫化鈉法制備的電極的性能。但是考慮到敏感膜與金屬基體之間的附著作用,硫代乙酰胺法制備的電極硫化程度更高與基體之間的結(jié)合更加緊密,因而更適合使用在特殊環(huán)境下使用。(3)在模擬海洋環(huán)境中的應(yīng)用:制備出適合檢測(cè)海洋離子的金汞齊電極,并應(yīng)用于Mn2+、Cu2+和S2-等多種離子的檢測(cè)。同時(shí)將電極應(yīng)用到在高達(dá)80℃的環(huán)境中進(jìn)行應(yīng)用,仍然能獲得較好的溶出伏安曲線。因此金汞齊電極具有高溫環(huán)境下工作的應(yīng)用前景。并將前期制備的Ir/Ir02 pH和Ag/Ag2S H2S電極在高達(dá)150℃的高溫高壓下進(jìn)行測(cè)試。實(shí)驗(yàn)結(jié)果表明:所制備的電極內(nèi)對(duì)溫度和濃度的變化呈現(xiàn)出較理想的能斯特響應(yīng),可以初步應(yīng)用于高溫高壓環(huán)境。
[Abstract]:In 21th century, the ocean century, the study of various physical and chemical properties in the marine environment is related to the survival and development of human beings. In situ testing can timely feedback changes in the physical and chemical parameters of the test environment. Therefore, it is a hot topic for the scholars to study the ocean. In this paper, we have prepared several kinds of characteristics, such as small size, simple operation, easy to miniaturize, high sensitivity, in situ testing and so on. The electrochemical sensor which can be used in marine environment testing, the main contents are as follows: 1) the Ir/IrO2 pH electrode was prepared by melting carbonate method and NaOH cyclic thermal oxidation method. The surface morphology, composition content, response time, reversibility and stability of the electrode were analyzed. It is considered that NaOH cyclic thermal oxidation is a more suitable method for preparing Ir/IrO2 electrode. It is the first time to improve the stability of the electrode by the method of hydrothermal treatment. The experimental results show that the electrode after hydrothermal treatment has a fast response rate of 3sN, high sensitivity of 70.5 MV / pH ~ (-1) and good reproducibility. Small lag, long service life and so on. In more than a month of continuous testing. The potential drift is less than 5 MV. The method of hydrothermal treatment effectively solves the phenomenon of potential drift of Ir/IrO2 pH electrode for a long time. The stability of the electrode was improved. (2) Ag wire was used as the metal matrix and sodium sulfide method was used respectively. Dipping silver paste and thioacetamide CH3CSNH2). The preparation method of Ag/AgaS electrode suitable for marine environment was selected. The experimental results showed that the electrode prepared by the latter two methods had a fast response rate. Because of its high sensitivity and wide detection range, the performance of the electrode prepared by sodium sulphide method is improved effectively, but the adhesion between the sensitive film and the metal substrate is considered. The sulfidation degree of the electrode prepared by thioacetamide method is higher than that of the substrate. Therefore, it is more suitable for use in special environment. 3) in simulated marine environment: the gold amalgam electrode suitable for ocean ion detection is prepared and applied to Mn2. Cu2 and S2- are used to detect many kinds of ions. At the same time, the electrode is applied in the environment as high as 80 鈩，

本文編號(hào)：1373008